SHORT PROCEDURE FOR CHEMISTRY LABORATORY

DEPARTMENT OF CHEMISTRY

Estimation of the Ferrous ion by potentiometry

, and Csolutions are made up to exactly 100ml using standard measuring flask.
The given A
Contents Titration I
Title E s t i m a t i o n F e r r o u s ion

Burette solution Standardized K,Cr, 0, (C)

Pipette solution 20ml of Standard FeSO, (B)
Condition One test tube full of dil. H,50.
Electrochemical cell is constructed by using :
Electrodes used .i Reference electrode: Saturated calomel
ii. Indicator electrode : Pt electrode
rod. Emf of the cell si noted with
Experimental Electrodes are immersed ni beaker solution along with glass
setup the progressive addition of K,Cr,07.

Observation Every increment of KC t nearby equivalence point, sudden

, r, 0, emf of hte cel increases. A
increase in the emf is observed

Model Graphs

- …

Calculation Equivalent weight of Fe'* is 55.45, FeSO, si 278.

* ~ (0 )
Amont:
1000 ( 4 )

55-85 x
1000 、
 NaCK=.
Normality
= Ne ma lit y * a n Rublind
Estimation of the strength of acids by conductometry
The given A, and C solutions are made up to exactly 100ml using 100ml standard measuri
ng flask.
Contents Ti t r a t i o n I
Title Estimation of the strength of Acid
Burette s o l u t i o n Standardized NaOH (C)
Pipette solution 40ml of Standard H,SO, acid (B)
Electrodes used Conductivity cell si made of two platinized platinum electrodes separated at a fixed
distance.

Experimental setup Conductivity cell si immersed ni beaker solution along with glass rod. Conductance of the
Observation
sulution si noted with the progressive addition of NaOH.
Every increment of NaOH, the conductance of the solution decreases. At nearby
equivalence point, increasing trend of the conductance observed.

Model Graphs
트

Calculation Equivalent weight of H,SO,, HCl and CH,COOH are 49, 36.45 and 60 respectively.

= V,N,

Amant: E h mality sin

24.wk: H2504: 49: 0

 Electroplating of Nickel / copper and Determination of cathodic efficiency
Foilowing steps are involved ni the electroplating and determination of cathodic efficiency of Ni plating:
1. Pretreatment Process 2. Electroplating Process
1. Polishing: The given 1. Initial weight of the
brass / stainless steel pretreated brass /
plates are polished stainless steel plates
with emery sheets was noted as W,.
and then washed 2. Ni-Plating: Pretreated
with running water plate is made as
dried and cooled cathode and Ni plates
2. Degreasing: The as anode in an
surfaces of the plates electrolytic cell
are degreased with containing suitable
acetone. electrolyte (NiSO,, NiCh,
3. Area to be electro and Boric acid buffer).
plated is fixed and Cu-Plating: Pretreated
c a l c u l a t e d in t e r m s of plate is made as
dm?' cathode and Copper as
4. Current to be passed B anode ni an electrolytic
a t t h e fixed c u r r e n t cell containing copper
density is calculated sulphate and sulphuric
Current = Current acid.
density x area. .3 Plate is immersed into
the electrolyte bath
ex b x 2 solution up to the mark
100 and calculated ampere
of current is passed
9 = 4x curert densi li
exactly for 15 minutes.
.4 After 15 minutes, the
plate is removed from
b a t h solution then
washed with running
water, dried, cooled
and weighed.
.5 Final weight of the
plate si noted as W2.
3. Determination of Cathode efficiency
.1 After electroplating, actual weight of the metal deposited
si calculated from the weights of the plates before (W,)
and after deposition (W.) plating.
.2 Theoretical weight of the nickel deposited si calculated
using the faradays first law of electrolysis:
m = zit
where,
m = mass of the metal deposited.
= electrochemical equivalent of the metal.
i = current in amperes
t = time in s e c o n d s
Cathode efficiency si calculated using the following
expression:
Cathode efficiency =
Actual weight of the metal deposiied
Theretical weight of the metal deposited X100
The experiment si repeated for remaining plates with the
same procedure at the given current densities.
Note:
For Nickel electroplating brass plates are used as cathode
For Copper electroplating stainless steel plates are used as
cathode.
Electrochemical equivalent = Equivalent weight of Nickel/ 965000C
of Nickel
Equivalent weight = Atomic weight/ valenes = 58.71/2 = 29.35
Electrochemical equivalem. 7. = 29.35/96500 = 03041x 10'g/ coulomb
Electrochemical equivalent =Liquivalent weight of copper/ 965000C
of copper
Equivalent weight = Atomic weight valency = 63.54/2 = 31.77
. = 31.77/96500 = 3.2901× 10* g/ coulomb
Electrochemical equivalent. Z
 and De ter m in ati on of thickness of anodic film
Anodising of Alumini um
alumi nium
dizing o f
Following steps are involved in the ano
Pr oc es s .
2 Anodising Process
.1 Pr et re at m en t
A l plates .1 Pre trea ted plate is
.1 Polishing: The give n pped by
made as anode and
are polished with emery
shee ts then was hed with Pb-Sb alloy sheets are
running water and dried m a d e c a t h o d e in an
electrolytic cell
2. Picking and decreasing: Given
plates are immersed in 5% conta ining suitable
electrolyte (40%
NaOH 1( mins) and washed
with running water. Followed H2504).
by neutralised with dil. HNO;, 2. Plate immersed into
again washed with running the electrolyte bath
w a t e r a n d dried solution upto the
3. Area to be anodized is fixed mark and definite
and calculated in terms of amp ere of DC curre nt
dn'
is passed exactly for
4. Current to be passed at the 15 minutes.
fixed curre nt dens ity is 3. After 15 minutes,
calculated. anodised plate is
Current = Current removed from bath
density(A/dm?) x area (dm}) solution t h e n w a s h e d
with running water,
dried cooled and
weighed (P1).
and de termi nation of thickness of oxide film:
.
3 De ter mi nat ion of Thickness of
ano dic film
d (P,).
.1 Initial weight of the anodized plate was note
.
2 Stripping: The anodized plate is then stri
dipping it in the solution of the following
° for 5 minutes.
composition, kept at 80 C
Ortho phosphoric acid - 32 ml
Chromic acid - 20g
Wa t e r - 1 liter.
3. Alter stripping, the plate is removed, washed, dried
and then weighed (P2). From the weight loss the
thickness of the anodic film is calculated using the
following expression:
0.1 ( P 1 - P 2 ) X 1.4
A =
3.42 F
where,
= the thickness of t h e film in microns.
(P,-P2) = the weight of the anodic film in mg.
= Coefficient to take into account the
1.4
porosity of the film.
3.42 = Specific gravity of the film
F = area of the anodized film in d m
The experiment is repeated for remaining plates with
the same procedure at the given current densities.
 =
EOTA
stersta
TA and lon exchange methods
Determination of total Hardness by ED n
Contents Titration I (EDTA) Method Titration I (lo
exchange)
tal
Estimation of Total Estimation of To
Title
Hardness hardness

Standardized EDTA Sodium hydroxide ( . )

Burette solution
Hard water
20ml of water sample (A)
10n)
Pipette solution

Condition 1 Test tube full of pH 10

buffer
Phenolphthalein
EBT (Erichrome Balck T)
Appearance of a
Indicator
e
Wi ne red to ste el blu
pink
permanent pale
End point
colour
50
, and CaCO, are 55.5 and
Calculation Equivalent weight of CaCk
respectively.

S): aker
L DISSOLVED SOLIDS (TD is transferred into the be
DETERMINATION OF TOTA 0 ml of the wa ter sam ple
weighed (w1). Exactly 2 idue is noted (w2). From
the difference
Aclean and dry beaker is the be ak er wi th the res
ss. The weight of
and evaporated to dryne pom
culated.
in weight, the TDS is cal 20
(Glass Electrode)
UR EM ENT F
O H
p OF GIVEN WATER SAMPLE:
MEAS ined glass and
ard bu ffer soluti on s of pH 4 and 11 using a comb
d using stand and the electrodes are
The pH meter is calibrate wa ter sam ple is taken in a clean beaker
of the given
calomel electrodes. 40ml ter.
is me asu red using a pHme
immersed in it and the pH
atinum Electrode)
REMENT F
O CONDUCTIVITY OF GIVEN WATER SAMPLE: (Pl
MEASU
of
using KI
C standard (0.01M KC I - conductivity 0.1413 mS/cm). 40ml
Aconductivity meter si calibrated ty cell connected to a conduc
tivity
in a clean beaker. The conductivi
the given water sample is taken conductivity of the water sample
is measured.
ersed into the sam ple and the
meter is imm

Calculation:
٧٠٢١
h a d w t w. N2;
N o m a li n m
5 0 x 11 0 0 = p p
Ammat (TO) hardress 5 1,0)=
 CTIC SYSTEM
TION F
O PHASE DIAGRAM FOR EUTE
CONSTRUC
bination f
o any two f
o the fatty acids: oleic,
a com
nstruct the phase diagram for a binary mixture, nt A and B and the following proced
ure is
o co
T acid is chosen as com
pone
a sensitive ich
itic and lauric bber cork through wh
stearic, myristic, palm wi th tw o- ho led ru
glass tube si fitted d transferred
followed. A clean hard g
1 of su bs tan ce A s
i weighed accurately an
r are inserted. Exactly heated till it melts com
pletely. The
thermometer and stirre d n
i a wa ter ba th and
tube is then immerse ced in a clean dry conical
flask
into the glass tube. The ce i
s wi pe d ou t and pla
bath, the water on its surfa first crystal appears si
tube si taken out of the tem pe rat ur e t
a wh ich , the
tant stirring. The freezing into the same tube. It is
again
and allowed to cool with cons ca ref ull y tra ns fer red
bstance B si weighed and then taken out and coole
d
noted. Exactly 0.1 g of su mo ge ne ou s liqu id. It s
i
the mixture becomes a ho ent is rep ea ted several
tim es by
heated ni the hot bath till s
i no ted . The ex pe rim
ng point of the mixture ed into the
with stirring. The freezi
ble .
)
I About 1 gra ms o f sub stance Bis accurately weigh
to A(Ta experiment is repeated
by
adding 0.1 g of B, each time mi ne d as bef ore . Th e
the freezing point is deter xis and
second boiling-tube and
. l
I.
) A gra ph s
i plo tted by tak in?, composition along the x-a
to B(Table freezing point of A with
adding 0.1 g of Aeach time wi ng the ch an ce n
i the
axis. Two curves, one sho pect to the addition
temperature along the y
the other showin g the freezing point of Bwith res
respect to the addition of ntB, and
at which the two curves me
et gives the eutectic point of
the binary system
of A are obtained. The poi
ect ic com pos itio n is obtained.
A and B fro m which the eut
al
a binary mixture i
n which tie t o components are miscible in
Eutectics:. A eutectic system si
lten) sta te
proportion in the liquid (mo
react chemically
1. The two com po nen ts do not ntg point.
ty of lowering the other's
2. Each component has the proper point of all the
two compon ent eutectic system, which has the lowest freezing
3. Amixture of the ture.
, is known as eutectic
possible mixtures of the components mixture is known as
freezing point attainable correspondingot u t e c t i c
4. The minimum
eutectic point.
Model graph
TIC
TIC
T, •
Liquid (L)
T,

i
u+E
Solid Solid

100° A - Composition (st